WO2011108356A1 - Method for producing silicon carbide crystal, silicon carbide crystal, and device for producing silicon carbide crystal - Google Patents
Method for producing silicon carbide crystal, silicon carbide crystal, and device for producing silicon carbide crystal Download PDFInfo
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- WO2011108356A1 WO2011108356A1 PCT/JP2011/053273 JP2011053273W WO2011108356A1 WO 2011108356 A1 WO2011108356 A1 WO 2011108356A1 JP 2011053273 W JP2011053273 W JP 2011053273W WO 2011108356 A1 WO2011108356 A1 WO 2011108356A1
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/36—Carbides
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B23/00—Single-crystal growth by condensing evaporated or sublimed materials
- C30B23/02—Epitaxial-layer growth
- C30B23/06—Heating of the deposition chamber, the substrate or the materials to be evaporated
- C30B23/063—Heating of the substrate
Definitions
- the present invention relates to a method for manufacturing a silicon carbide (SiC) crystal, an SiC crystal, and an apparatus for manufacturing an SiC crystal.
- SiC silicon carbide
- the SiC crystal has a large band gap, and the maximum breakdown electric field and thermal conductivity are larger than those of silicon (Si), while the carrier mobility is as large as that of Si, and the saturation drift velocity and withstand voltage of electrons are also high. large. Therefore, application to a semiconductor device that is required to have high efficiency, high breakdown voltage, and large capacity is expected.
- FIG. 6 is a cross-sectional view schematically showing a SiC manufacturing apparatus disclosed in Non-Patent Document 1. The SiC crystal manufacturing apparatus and growth method disclosed in Non-Patent Document 1 will be described with reference to FIG.
- the SiC manufacturing apparatus disclosed in Non-Patent Document 1 includes a crucible 101 and a heat insulating material 121 that covers the outer periphery of the crucible 101. Under the crucible 101, an SiC crystal material 17 is disposed. On top of the crucible 101, the seed crystal 11 is disposed so as to face the raw material 17.
- the heat insulating material 121 is formed on the side of the seed crystal 11 arranged inside the crucible 101, on the side of the raw material 17 arranged inside the crucible 101, with an opening 121 a formed so as to penetrate to the outer periphery of the heat insulating material 121, And an opening 121b formed so as to penetrate to the outer periphery of the heat insulating material 121.
- the raw material 17 is heated to a temperature at which the raw material 17 sublimes.
- the raw material 17 is sublimated to generate a sublimation gas, and an SiC crystal grows on the surface of the seed crystal 11 installed at a lower temperature than the raw material 17.
- Non-Patent Document 1 when the heat insulating material 121 has the opening 121a on the seed crystal 11 side, heat can be released at the time of starting the growth of the SiC crystal, so the temperature of the opening 121a becomes lower. However, when the source gas leaking from the crucible 101 adheres, the temperature of the opening 121a is low, and thus SiC crystals adhere to the opening 121a. For this reason, the opening 121a may be buried. If the opening 121a opened in the heat insulating material 121 is buried during the growth, the growth conditions change. For this reason, the crystallinity of the growing SiC crystal is deteriorated.
- the present invention relates to an SiC crystal manufacturing method, an SiC crystal, and an SiC crystal manufacturing apparatus capable of improving the crystallinity of the SiC crystal.
- the SiC crystal manufacturing method of the present invention includes the following steps.
- a manufacturing apparatus including a crucible and a heat insulating material covering the outer periphery of the crucible is prepared.
- the raw material is placed in the crucible.
- a seed crystal is arranged so as to face the raw material.
- the raw material is heated to be sublimated, and a raw material gas is deposited on the seed crystal to grow a silicon carbide (SiC) crystal.
- the process of preparing a manufacturing apparatus includes the process of arrange
- the SiC crystal manufacturing apparatus of the present invention is an apparatus for growing a SiC crystal by sublimating a raw material containing SiC and precipitating the sublimated raw material gas on a seed crystal. And a heating unit.
- a crucible arranges a raw material and a seed crystal inside.
- the heat insulating material covers the outer periphery of the crucible.
- the heat dissipating part is disposed between the outer surface of the crucible on the seed crystal side and the heat insulating material, and consists of a space.
- the heating unit heats the inside of the crucible.
- the heat radiation part on the outer surface of the crucible on the seed crystal side is covered with the heat insulating material.
- the heat insulating material can suppress that the gas which leaked from the crucible mixes in a thermal radiation part.
- a thermal radiation part is buried in the growth of a SiC crystal.
- the heat dissipating part can be maintained as a space, heat on the seed crystal side of the crucible can be released to the outside of the manufacturing apparatus by heat conduction by radiation at the growth temperature of the SiC crystal. For this reason, it can suppress that the temperature of a seed crystal changes during the growth of a SiC crystal. Therefore, it is possible to suppress the growth conditions from changing during the growth of the SiC crystal, and hence the crystallinity of the SiC crystal can be improved.
- a heat insulating material mainly composed of carbon (C) is prepared in the step of preparing the manufacturing apparatus.
- the heat insulating material preferably contains C as a main component.
- a manufacturing apparatus for covering the outer periphery of the crucible with a heat insulating material in which a plurality of heat insulating sheets are laminated is prepared.
- the heat insulating material includes a plurality of heat insulating sheets laminated.
- a heat radiating portion can be easily formed by providing an opening in at least one of the plurality of heat insulating sheets and covering the opening with another heat insulating sheet.
- the raw material is heated by a high-frequency heating method or a resistance heating method.
- the heating unit is preferably a high-frequency heating coil or a resistance heater.
- the high-frequency heating coil and the resistance heater are easy to control the temperature, the temperature change during the growth of the SiC crystal can be suppressed. For this reason, the crystallinity of the SiC crystal can be improved.
- a crucible mainly containing C is prepared in the step of preparing the manufacturing apparatus.
- the crucible contains C as a main component.
- the SiC crystal of the present invention is manufactured by any of the above-described SiC crystal manufacturing methods. Since the SiC crystal of the present invention is manufactured while suppressing changes in growth conditions during crystal growth, the crystallinity can be improved.
- the crystal polymorph (polytype) is preferably 4H—SiC.
- the material of a device with a high breakdown voltage can be realized.
- the SiC crystal manufacturing method, the SiC crystal, and the SiC crystal manufacturing apparatus of the present invention since the change of the growth conditions can be suppressed during the growth of the SiC crystal by the heat dissipation portion, the crystallinity of the SiC crystal is improved. be able to.
- SiC crystal 10 according to an embodiment of the present invention will be described.
- the SiC crystal 10 has good crystallinity.
- the polytype of the SiC crystal 10 is not particularly limited, but is preferably 4H—SiC.
- This manufacturing apparatus 100 is an apparatus for growing SiC crystals by a sublimation method. That is, the manufacturing apparatus 100 is an apparatus for growing the SiC crystal 10 by sublimating the raw material 17 containing SiC and precipitating the sublimated source gas on the seed crystal 11.
- the manufacturing apparatus 100 mainly includes a crucible 101, a heat insulating material 121, a reaction vessel 123, a heating unit 125, and a heat dissipation unit 131.
- the crucible 101 arranges the seed crystal 11 and the raw material 17 inside.
- the crucible 101 preferably contains C as a main component, and more preferably contains C as a main component and the remainder is made of inevitable impurities.
- the crucible 101 is made of a material that is stable under the growth conditions of the SiC crystal, changes in the growth conditions during the growth of the SiC crystal can be suppressed. For this reason, the crystallinity of the SiC crystal to be manufactured can be improved.
- the crucible 101 is preferably made of graphite, for example. Since graphite is stable at high temperatures, cracking of the crucible 101 can be suppressed.
- C constituting the crucible 101 is a constituent element of the SiC crystal, even if the crucible 101 is sublimated and mixed into the SiC crystal, it can be suppressed from becoming an impurity. For this reason, the crystallinity of the SiC crystal to be manufactured can be improved.
- the heat insulating material 121 covers the outer periphery of the crucible 101.
- the heat insulating material 121 is preferably composed mainly of C, more preferably composed of C as a main component, and the remainder composed of inevitable impurities.
- the heat insulating material is preferably made of carbon felt, for example. Also in this case, since it has a heat insulation effect and the change of the growth conditions during the growth of the SiC crystal can be suppressed, the crystallinity of the manufactured SiC crystal can be improved.
- a temperature measuring hole 121 c is formed on the raw material 17 side of the heat insulating material 121.
- the heat radiating part 131 is disposed between the outer surface 101 a of the crucible 101 on the seed crystal 11 side and the heat insulating material 121.
- the heat radiating part 131 is formed so as to be in contact with the outer surface 101a (the outer surface 101a on the back side of the surface on which the seed crystal 11 is disposed) facing the inner surface on which the seed crystal 11 is disposed in the crucible 101.
- the heat radiating portion 131 is a space formed between the crucible 101 and the heat insulating material 121 covering the outer surface 101a of the crucible 101 on the seed crystal 11 side.
- the heat dissipation part 131 is a space. This space is filled with an atmospheric gas such as nitrogen (N 2 ) gas, helium (He) gas, or argon (Ar) gas during the growth of the SiC crystal.
- an atmospheric gas such as nitrogen (N 2 ) gas, helium (He) gas, or argon (Ar) gas during the growth of the SiC crystal.
- the center of the heat radiation part 131 and the center of the crucible 101 coincide. In this case, variation in the heat transfer in the lateral direction of the seed crystal 11 can be suppressed.
- the heat radiation part 131 preferably includes all regions where the seed crystal 11 to be arranged is projected onto the outer surface 101a of the crucible 101 when viewed from the raw material 17 side. In this case, the effect of increasing the in-plane uniformity of temperature due to the heat radiation from the heat radiation portion 131 is high.
- the heat radiating part 131 may include a part of the region where the seed crystal 11 to be arranged is projected onto the outer surface 101a of the crucible 101 as viewed from the raw material 17 side, or may not include the entire region. Good.
- the seed crystal 11 to be arranged may include all the regions in which the heat radiation part 131 is projected onto the outer surface 101a of the crucible 101 when viewed from the raw material 17 side.
- a reaction vessel 123 is provided around the heat insulating material 121. At both ends of the reaction vessel 123, for example, a gas introduction port 123a for flowing atmospheric gas into the reaction vessel 123 and a gas discharge port 123b for discharging atmospheric gas to the outside of the reaction vessel 123 are formed. .
- a heating unit 125 for heating the inside of the crucible 101 is provided on the outer side of the crucible 101 (in this embodiment, the outer central portion of the reaction vessel 123).
- the heating unit 125 is not particularly limited, but is preferably a high frequency heating coil or a resistance heater.
- a high frequency heating coil is installed in the outer periphery of the heat insulating material 121.
- FIG. When a resistance heater is used as the heating unit 125, the resistance heater is preferably installed inside the heat insulating material 121 and outside the crucible 101.
- thermometers 127b and 127a for measuring the temperature above and below the crucible 101 are provided.
- the radiation thermometer 127a is measured through a temperature measuring hole 121c formed in a part of the heat insulating material 121 covering the outer surface 101b on the raw material 17 side of the crucible 101.
- the temperature measuring hole 121c may not be formed.
- the manufacturing apparatus of Modification 1 shown in FIG. 3 basically has the same configuration as the manufacturing apparatus 100 shown in FIG. 2, but the outer surface 101 b on the raw material 17 side of the crucible 101 and the heat insulating material 121. There is a difference in that a heat dissipating part 132 made of a space is further formed between them and a temperature measuring hole 121c is not formed in the heat insulating material 121.
- the manufacturing apparatus of Modification 2 shown in FIG. 4 basically has the same configuration as that of the manufacturing apparatus 100 shown in FIG. 2, but differs in that the temperature measuring hole 121 c is not formed in the heat insulating material 121.
- the manufacturing apparatus 100 may include various elements other than those described above, but illustration and description of these elements are omitted for convenience of description.
- a manufacturing apparatus 100 including a crucible 101 and a heat insulating material 121 covering the outer periphery of the crucible 101 is prepared.
- a heat dissipating part 131 made of a space is disposed between the outer surface 101 a of the crucible 101 on the side where the seed crystal 11 is located and the heat insulating material 121.
- the manufacturing apparatus 100 shown in FIGS. 2 to 4 is prepared.
- a heat insulating material 121 mainly composed of C. It is preferable to prepare a crucible 101 containing C as a main component. It is preferable to arrange a heating unit 125 that is a high-frequency heating coil or a resistance heater.
- the manufacturing apparatus 100 that covers the outer periphery of the crucible 101 with a heat insulating material 121 in which a plurality of heat insulating sheets are laminated.
- a heat insulating material 121 in which a plurality of heat insulating sheets are laminated.
- holes are formed in at least one of the plurality of heat insulating sheets, the heat insulating sheet having the holes formed therein is disposed so as to contact the crucible 101, and the remaining heat insulating sheets are disposed so as to cover the holes.
- the hole of the heat insulation sheet becomes the heat radiating part 131.
- the raw material 17 is placed in the crucible 101.
- the raw material 17 may be a powder or a sintered body.
- a polycrystalline SiC powder or a SiC sintered body is prepared.
- the raw material 17 is installed below the crucible 101.
- the seed crystal 11 is arranged in the crucible 101 so as to face the raw material 17.
- seed crystal 11 is arranged on top of crucible 101 so as to face raw material 17.
- the crystal structure of the seed crystal 11 is not particularly limited, and may be the same crystal structure as the growing SiC crystal or a different crystal structure. From the viewpoint of improving the crystallinity of the growing SiC crystal, it is preferable to prepare an SiC crystal having the same crystal structure as the seed crystal 11.
- the raw material 17 is sublimated by heating, and a raw material gas is deposited on the seed crystal 11 to grow an SiC crystal.
- the raw material 17 is heated by the heating unit 125 to a temperature at which the raw material 17 sublimes.
- the heating method is not particularly limited, but it is preferable to use a high-frequency heating method or a resistance heating method.
- the raw material 17 is sublimated to generate a sublimation gas (raw material gas).
- This sublimation gas is solidified again on the surface of the seed crystal 11 installed at a lower temperature than the raw material 17.
- the growth temperature for example, the temperature of the raw material 17 is maintained at 2300 ° C. to 2400 ° C., and the temperature of the seed crystal 11 is maintained at 2100 ° C. to 2200 ° C. Thereby, a SiC crystal grows on the seed crystal 11.
- the heat radiation part 131 is filled with the atmospheric gas flowing from the gas inlet 123a of the reaction vessel 123 into the reaction vessel 123.
- heat conduction by radiation by the heat radiating portion 131 becomes dominant. Therefore, heat can be radiated from the outer surface 101a on the side where the seed crystal 11 is disposed in the crucible 101 by the heat radiating portion 131.
- the heat radiating portion 131 is covered with the heat insulating material 121, it is possible to suppress the SiC crystal from being deposited inside the heat radiating portion 131 even if the growth of the SiC crystal is continued. Therefore, changes in growth conditions such as a change in the temperature of the seed crystal 11 can be suppressed while growing the SiC crystal. Therefore, it is possible to grow a SiC crystal with good crystallinity, such as producing an intended polytype SiC crystal.
- the inside of the manufacturing apparatus 100 is cooled to room temperature. Then, the manufactured SiC crystal is taken out from the manufacturing apparatus 100. Thereby, the SiC crystal 10 (SiC ingot) shown in FIG. 1 provided with the seed crystal 11 and the SiC crystal formed on the seed crystal 11 can be manufactured.
- the SiC crystal 10 shown in FIG. 1 may be manufactured by removing the seed crystal 11 from the SiC ingot. When removing, only the seed crystal 11 may be removed, or a part of the seed crystal 11 and the grown SiC crystal may be removed.
- the removal method is not particularly limited, and a mechanical removal method such as cutting, grinding, and cleavage can be used.
- Cutting refers to mechanically removing at least the seed crystal 11 from the SiC ingot with a slicer having an outer peripheral edge of an electrodeposited diamond wheel.
- Grinding refers to scraping in the thickness direction by contacting the surface while rotating the grindstone.
- Cleaving means dividing the crystal along the crystal lattice plane.
- a chemical removal method such as etching may be used.
- the SiC crystal 10 shown in FIG. 1 may be manufactured by cutting a plurality of SiC crystals from the grown SiC crystal. In this case, the manufacturing cost of one SiC crystal 10 can be reduced.
- one or both surfaces of the crystal may be flattened by grinding or polishing.
- the SiC crystal manufacturing apparatus of the comparative example shown in FIG. 5 has basically the same configuration as the manufacturing apparatus 100 of the present embodiment shown in FIG. Different in. That is, the manufacturing apparatus of the comparative example covers the entire surface of the crucible 101 including the outer surface 101 a on the seed crystal 11 side with the heat insulating material 121.
- the temperature of the seed crystal 11 gradually increases because the inside of the crucible 101 is heated to a high temperature. For this reason, it is difficult to appropriately control the sublimation gas of the raw material 17 to deposit it on the seed crystal 11 side, and it becomes difficult to grow the SiC crystal.
- the SiC crystal manufacturing apparatus of Non-Patent Document 1 shown in FIG. 6 has basically the same configuration as the manufacturing apparatus 100 of the present embodiment shown in FIG. It differs in that it is a through-hole 121a provided in the material 121.
- Non-Patent Document 1 since heat can be released from the opening 121a at the initial stage of SiC crystal growth, the temperature of the seed crystal 11 located on the opening 121a side is lowered. However, when the source gas leaked from the crucible 101 flows in the growth of the SiC crystal, the temperature of the opening 121a is low, so that the crystal adheres to the opening 121a. For this reason, the opening part 121a provided in the heat insulating material 121 is buried during the growth of the SiC crystal. As a result, the growth temperature of the SiC crystal changes during the growth. For this reason, crystallinity deteriorates, for example, the polytype of the growing SiC crystal changes from the intended one.
- the heat dissipating part 131 disposed on the outer surface 101a of the crucible 101 on the seed crystal 11 side is formed of the heat insulating material 121. Covering. Thereby, even when gas leaks from the crucible 101 and enters the heat radiating portion 131, the temperature drop of the heat radiating portion 131 can be suppressed, so that SiC crystals are deposited on the heat radiating portion 131 (that is, the heat radiating portion 131 is (Filling with SiC crystal) can be suppressed.
- the present inventor has found that heat conduction by radiation generated by forming the heat dissipating part 131 becomes dominant under the high temperature conditions for growing the SiC crystal. For this reason, in this Embodiment, since the thermal radiation part 131 can be maintained as space in the growth of a SiC crystal, in the growth temperature of a SiC crystal, the heat of the seed crystal 11 side of the crucible 101 is conducted by heat conduction by radiation. Can be released to the outside. That is, the heat radiation from the crucible 101 can be largely maintained through the heat radiation part 131. For this reason, since the temperature of the seed crystal 11 can be suppressed during the growth of the SiC crystal, the temperature of the seed crystal 11 can be maintained lower than the temperature of the raw material 17.
- the difference between the temperature of the seed crystal 11 at the initial growth stage of the SiC crystal and the temperature of the seed crystal 11 at the middle growth stage (or the final stage) can be made smaller than that in Non-Patent Document 1. Therefore, since a change in growth conditions such as a change in the temperature of the seed crystal 11 can be suppressed during the growth of the SiC crystal, a SiC crystal with good crystallinity can be manufactured.
- Invention Examples 1 and 2 In Invention Examples 1 and 2, a SiC crystal was manufactured using the manufacturing apparatus 100 of the above-described embodiment shown in FIG. 2 according to the manufacturing method of the above-described embodiment.
- a hollow cylindrical crucible 101 made of graphite was prepared.
- the outer diameter of the crucible 101 was 140 mm, the inner diameter was 120 mm, and the height was 100 mm.
- three heat insulating sheets each having a thickness of 10 mm and made of carbon felt were prepared.
- two heat insulating sheets were formed with openings having an outer diameter of 20 mm in Invention Example 1 and an outer diameter of 30 mm in Invention Example 2, respectively.
- the two heat insulation sheets in which the opening part was formed were arrange
- the center of the opening and the center of the crucible 101 were matched.
- the heat radiating part 131 a space surrounded by the opening formed in the two heat insulating sheets and the heat insulating sheet in which the opening was not formed was formed.
- the heat dissipating part 131 made of a space was disposed between the outer surface 101 a of the crucible 101 on the seed crystal 11 side and the heat insulating material 121.
- the heat insulating sheet constituted the heat insulating material 121.
- the crucible 101, the heat radiating part 131, and the heat insulating material 121 were accommodated inside the reaction container 123, and a high-frequency heating coil as the heating part 125 was disposed on the outer periphery of the reaction container 123.
- the raw material 17 was arranged at the lower part in the crucible 101.
- the raw material 17 used SiC powder.
- seed crystal 11 was arranged in the upper part of crucible 101 so as to face raw material 17.
- 4H—SiC having an outer diameter of 75 mm was used as the seed crystal 11.
- He gas having a flow rate of 0.5 slm and N 2 gas having a flow rate of 0.1 slm are allowed to flow into the reaction vessel 123 as the atmospheric gas, and the temperature in the crucible 101 is measured using a high-frequency heating coil as the heating unit 125.
- the temperature was raised.
- the pressure in the crucible 101 was set to 20 Torr.
- the power of the high-frequency heating coil was controlled so that the temperature on the seed crystal 11 side was lower than the temperature on the raw material 17 side, for example, 2200 ° C.
- SiC gas was sublimated from the raw material 17, and the SiC crystal was grown on the seed crystal 11 with a growth time of 50 hours.
- the intended polytype was 4H—SiC. Thereafter, the temperature inside the manufacturing apparatus 100 was cooled to room temperature. Thereby, the SiC crystal was manufactured.
- Comparative Examples 1 to 5 The SiC crystal manufacturing apparatus and manufacturing method of Comparative Examples 1 to 5 were basically the same as those of Examples 1 and 2 of the present invention, but differed in that the heat dissipating part penetrated the heat insulating material. Specifically, all the three heat insulating sheets are provided with openings of the same size described in Table 1 below, and as shown in FIG. 6, the openings are overlapped to penetrate the heat insulating material. 121a was formed. In Comparative Examples 1 to 5, the opening 121b formed so as to penetrate to the outer periphery of the heat insulating material 121 was not formed on the raw material 17 side of the crucible 101.
- the SiC crystal having improved crystallinity by disposing the heat dissipating part 131 formed of a space between the outer surface 101a on the seed crystal 11 side of the crucible 101 and the heat insulating material 121. It was confirmed that can be manufactured.
Abstract
Description
本発明例1および2では、図2に示す上述した実施の形態の製造装置100を用いて、上述した実施の形態の製造方法にしたがって、SiC結晶を製造した。 (Invention Examples 1 and 2)
In Invention Examples 1 and 2, a SiC crystal was manufactured using the
比較例1~5のSiC結晶の製造装置および製造方法は、基本的には本発明例1および2と同様であったが、放熱部が断熱材を貫通している点において異なっていた。具体的には、3枚の断熱シートすべてに下記の表1に記載の同じ大きさの開口部を設け、図6に示すように、それぞれの開口部を重ねて、断熱材を貫通する開口部121aを形成した。なお、比較例1~5には、坩堝101の原料17側に、断熱材121の外周まで貫通するように形成された開口部121bは形成しなかった。 (Comparative Examples 1 to 5)
The SiC crystal manufacturing apparatus and manufacturing method of Comparative Examples 1 to 5 were basically the same as those of Examples 1 and 2 of the present invention, but differed in that the heat dissipating part penetrated the heat insulating material. Specifically, all the three heat insulating sheets are provided with openings of the same size described in Table 1 below, and as shown in FIG. 6, the openings are overlapped to penetrate the heat insulating material. 121a was formed. In Comparative Examples 1 to 5, the
比較例1~5について、SiC結晶を成長する前の放熱部(開口部)の面積に対して、SiC結晶を成長した後の閉塞した放熱部(開口部)の面積の割合(閉塞率)を求めた。その結果を下記の表1に記載する。 (Measuring method)
For Comparative Examples 1 to 5, the ratio (blocking rate) of the area of the heat radiation portion (opening) closed after growing the SiC crystal to the area of the heat radiation portion (opening) before growing the SiC crystal Asked. The results are listed in Table 1 below.
表1に示すように、坩堝101の種結晶11側の外表面101aと、断熱材121との間に、空間からなる放熱部131を配置した本発明例1および2の製造装置100および製造方法では、50時間のSiC結晶の成長の間、放熱部131が埋まることはなかった。このため、SiC結晶の成長中に成長条件が変化することを抑制できたので、成長したSiC結晶から切り出したSiC結晶基板には、ポリタイプ異常のものが1枚も含まれていなかった。 (Measurement result)
As shown in Table 1, the
Claims (12)
- 坩堝(101)と、前記坩堝(101)の外周を覆う断熱材(121)とを含む製造装置(100)を準備する工程と、
前記坩堝(101)内に原料(17)を配置する工程と、
前記坩堝(101)内において、前記原料(17)と対向するように種結晶(11)を配置する工程と、
前記坩堝(101)内において、前記原料(17)を加熱することにより昇華させて、前記種結晶(11)に原料ガスを析出することにより炭化珪素結晶(10)を成長する工程とを備え、
前記製造装置(100)を準備する工程は、前記坩堝(101)の前記種結晶(11)側の外表面(101a)と、前記断熱材(121)との間に、空間からなる放熱部(131,132)を配置する工程を含む、炭化珪素結晶(10)の製造方法。 Preparing a manufacturing apparatus (100) including a crucible (101) and a heat insulating material (121) covering the outer periphery of the crucible (101);
Placing the raw material (17) in the crucible (101);
Arranging the seed crystal (11) in the crucible (101) so as to face the raw material (17);
In the crucible (101), the step of growing the silicon carbide crystal (10) by sublimating the raw material (17) by heating and depositing the raw material gas on the seed crystal (11),
The step of preparing the manufacturing apparatus (100) includes a heat radiating part (space) between the outer surface (101a) of the crucible (101) on the seed crystal (11) side and the heat insulating material (121). 131, 132). A method for manufacturing a silicon carbide crystal (10), including a step of disposing 131, 132). - 前記製造装置(100)を準備する工程では、炭素を主成分とする前記断熱材(121)を準備する、請求項1に記載の炭化珪素結晶(10)の製造方法。 The method for manufacturing a silicon carbide crystal (10) according to claim 1, wherein in the step of preparing the manufacturing apparatus (100), the heat insulating material (121) mainly composed of carbon is prepared.
- 前記製造装置(100)を準備する工程では、複数枚の断熱シートを積層した前記断熱材(121)で、前記坩堝(101)の外周を覆う前記製造装置(100)を準備する、請求項1に記載の炭化珪素結晶(10)の製造方法。 In the step of preparing the manufacturing apparatus (100), the manufacturing apparatus (100) covering the outer periphery of the crucible (101) is prepared with the heat insulating material (121) obtained by laminating a plurality of heat insulating sheets. The manufacturing method of the silicon carbide crystal (10) as described in any one of.
- 前記炭化珪素結晶(10)を成長する工程では、高周波加熱法または抵抗加熱法により前記原料(17)を加熱する、請求項1に記載の炭化珪素結晶(10)の製造方法。 The method for producing a silicon carbide crystal (10) according to claim 1, wherein, in the step of growing the silicon carbide crystal (10), the raw material (17) is heated by a high-frequency heating method or a resistance heating method.
- 前記製造装置(100)を準備する工程では、炭素を主成分とする前記坩堝(101)を準備する、請求項1に記載の炭化珪素結晶(10)の製造方法。 The method for producing a silicon carbide crystal (10) according to claim 1, wherein, in the step of preparing the production apparatus (100), the crucible (101) containing carbon as a main component is prepared.
- 請求項1に記載の炭化珪素結晶(10)の製造方法により製造される、炭化珪素結晶(10)。 A silicon carbide crystal (10) produced by the method for producing a silicon carbide crystal (10) according to claim 1.
- 結晶多形が4H-SiCである、請求項6に記載の炭化珪素結晶(10)。 The silicon carbide crystal (10) according to claim 6, wherein the crystal polymorph is 4H-SiC.
- 炭化珪素を含む原料(17)を昇華させ、昇華させた原料ガスを種結晶(11)に析出させることにより炭化珪素結晶(10)を成長させる装置であって、
前記原料(17)および前記種結晶(11)を内部に配置するための坩堝(101)と、
前記坩堝(101)の外周を覆う断熱材(121)と、
前記坩堝(101)の前記種結晶(11)側の外表面(101a)と、前記断熱材(121)との間に配置され、空間からなる放熱部(131,132)と、
前記坩堝(101)の内部を加熱するための加熱部(125)とを備えた、炭化珪素結晶(10)の製造装置(100)。 An apparatus for growing a silicon carbide crystal (10) by sublimating a raw material (17) containing silicon carbide and precipitating a sublimated raw material gas on a seed crystal (11),
A crucible (101) for disposing the raw material (17) and the seed crystal (11) inside;
A heat insulating material (121) covering the outer periphery of the crucible (101);
A heat dissipating part (131, 132) composed of a space disposed between the outer surface (101a) of the crucible (101) on the seed crystal (11) side and the heat insulating material (121);
An apparatus (100) for producing a silicon carbide crystal (10), comprising a heating section (125) for heating the inside of the crucible (101). - 前記断熱材(121)は、炭素を主成分とする、請求項8に記載の炭化珪素結晶(10)の製造装置(100)。 The said heat insulating material (121) is a manufacturing apparatus (100) of the silicon carbide crystal (10) of Claim 8 which has carbon as a main component.
- 前記断熱材(121)は複数枚の断熱シートが積層されている、請求項8に記載の炭化珪素結晶(10)の製造装置(100)。 The said heat insulating material (121) is a manufacturing apparatus (100) of the silicon carbide crystal (10) of Claim 8 with which the several heat insulation sheet | seat is laminated | stacked.
- 前記加熱部(125)は、高周波加熱コイルまたは抵抗加熱ヒータである、請求項8に記載の炭化珪素結晶(10)の製造装置(100)。 The said heating part (125) is a manufacturing apparatus (100) of the silicon carbide crystal (10) of Claim 8 which is a high frequency heating coil or a resistance heater.
- 前記坩堝(101)は、炭素を主成分とする、請求項8に記載の炭化珪素結晶(10)の製造装置(100)。 The said crucible (101) is a manufacturing apparatus (100) of the silicon carbide crystal (10) of Claim 8 which has carbon as a main component.
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CN2011800029199A CN102471930A (en) | 2010-03-02 | 2011-02-16 | Method for producing silicon carbide crystal, silicon carbide crystal, and device for producing silicon carbide crystal |
US13/376,457 US20120107218A1 (en) | 2010-03-02 | 2011-02-16 | Production method of silicon carbide crystal, silicon carbide crystal, and production device of silicon carbide crystal |
EP11750469.6A EP2543753A4 (en) | 2010-03-02 | 2011-02-16 | Method for producing silicon carbide crystal, silicon carbide crystal, and device for producing silicon carbide crystal |
CA2765856A CA2765856A1 (en) | 2010-03-02 | 2011-02-16 | Production method of silicon carbide crystal, silicon carbide crystal, and production device of silicon carbide crystal |
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JP2015013762A (en) * | 2013-07-03 | 2015-01-22 | 住友電気工業株式会社 | Method of manufacturing silicon carbide single crystal, and silicon carbide single crystal substrate |
JP6438951B2 (en) * | 2013-07-26 | 2018-12-19 | トゥー‐シックス・インコーポレイテッド | Method for synthesizing ultra-high purity silicon carbide |
CN104477917B (en) * | 2014-11-20 | 2016-08-24 | 江苏乐园新材料集团有限公司 | Silicon carbide smelting method |
JP2016098157A (en) * | 2014-11-25 | 2016-05-30 | 住友電気工業株式会社 | Method for producing silicon carbide single crystal |
JP6462857B2 (en) * | 2015-03-24 | 2019-01-30 | 昭和電工株式会社 | Method for producing silicon carbide single crystal |
CN108166058A (en) * | 2016-12-07 | 2018-06-15 | 上海新昇半导体科技有限公司 | 4H-SiC growing methods |
JP7094171B2 (en) * | 2018-07-18 | 2022-07-01 | 昭和電工株式会社 | Method for manufacturing SiC single crystal |
JP7242987B2 (en) | 2018-09-06 | 2023-03-22 | 株式会社レゾナック | SiC single crystal manufacturing equipment |
JP7129856B2 (en) | 2018-09-06 | 2022-09-02 | 昭和電工株式会社 | Crystal growth device |
JP7057014B2 (en) * | 2020-08-31 | 2022-04-19 | セニック・インコーポレイテッド | A method for manufacturing a silicon carbide ingot and a silicon carbide ingot manufactured by the method. |
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